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CN-121990989-A - Preparation method of N-acetyl cerulosa and application of N-acetyl cerulosa prepared by preparation method in fabric dyeing

CN121990989ACN 121990989 ACN121990989 ACN 121990989ACN-121990989-A

Abstract

The invention discloses a preparation method of N-acetyl cerulosa and application of the N-acetyl cerulosa prepared by the preparation method in fabric dyeing, and relates to the technical field of compound synthesis. According to the preparation method of N-acetyl-blue, H 2 SO 4 and aluminum chloride are used as composite catalysts to catalyze the hydrolysis reaction of N, N '-diacetyl-blue, the potential barrier of the hydrolysis reaction of N, N' -diacetyl-blue can be reduced, one acetyl group in molecules is directionally removed, N-acetyl-blue is generated, and the product with the yield of more than 53% and the purity of more than 78% can be obtained by adopting the preparation method, and the purity and the reaction yield are excellent.

Inventors

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Assignees

  • 威兴蓝(江苏)新材料有限公司

Dates

Publication Date
20260508
Application Date
20260108

Claims (10)

  1. 1. The preparation method of the N-acetyl blue is characterized by comprising the following steps: Dispersing N, N '-diacetyl blue in water to obtain a reactant dispersion liquid, adding a composite catalyst to enable the N, N' -diacetyl blue to undergo hydrolysis reaction, then adding a terminator to terminate the reaction and separate out solid, and drying the solid after solid-liquid separation to obtain N-acetylyl blue; the composite catalyst comprises H 2 SO 4 and aluminum chloride; The terminator includes water at 0-5 ℃.
  2. 2. The method for preparing N-acetylblue according to claim 1, wherein the mass ratio of H 2 SO 4 to aluminum chloride in the composite catalyst is 1 (1.5-2.5).
  3. 3. The method for producing N-acetylblue according to claim 1 or 2, wherein the mass ratio of the composite catalyst to N, N' -diacetylblue is (0.01-0.02): 1.
  4. 4. The method for producing N-acetylblue according to claim 3, wherein the mass ratio of aluminum chloride to N, N' -diacetylblue is (0.007-0.012): 1.
  5. 5. The process for producing N-acetylblue according to claim 1, wherein the hydrolysis is carried out at a temperature of 15 to 35℃for a time of 1 to 2h ℃.
  6. 6. The process for producing N-acetylblue according to claim 5, wherein the hydrolysis is carried out at a temperature of 20 to 30℃for a period of 1.5 h.
  7. 7. The process for the preparation of N-acetylblue according to claim 1, wherein the mass ratio of N, N' -diacetylblue to water in the reactant dispersion is (0.4-0.6): 1.
  8. 8. The process for producing N-acetylblue according to claim 1 or 7, wherein the mass ratio of the terminator to the reactant dispersion is (2.8-5): 1.
  9. 9. The method for producing N-acetylblue according to claim 1, wherein the drying temperature is 60 to 90 ℃.
  10. 10. Use of N-acetyl blue prepared by the process of claims 1-7 for dyeing fabrics.

Description

Preparation method of N-acetyl cerulosa and application of N-acetyl cerulosa prepared by preparation method in fabric dyeing Technical Field The invention relates to the technical field of compound synthesis, in particular to a preparation method of N-acetyl cerulosa and application of the N-acetyl cerulosa prepared by the preparation method in fabric dyeing. Background Blue is one of the three primary colors of light, and its wavelength is relatively short, so blue light is one of the colors to which the human eye is sensitive, which also makes the application of blue pigments very wide. The blue dyes in the current market are of a wide variety, and most of the blue dyes are synthetic dyes, such as synthetic indigo, phthalocyanine blue, acid blue and the like. The hues of the dyes are different, the fastness and the performance are also greatly different, but in combination, most of the dyes can only reach the standard of one color fastness, and the requirements of multiple color fastnesses are difficult to meet. For example, the reactive Blue Turquoise Blue G has better soaping fastness but poor crockfastness. Chinese patent CN118756508a discloses N-acetyl cerulous blue as a dye obtained by structural modification of cerulous blue as a parent core, and has excellent soaping fastness and rubbing fastness. However, the current preparation method of N-acetyl cerulosa is mainly a microbial fermentation method, is complex and takes a long time, but a chemical method for directly carrying out structural modification on a cerulosa parent nucleus inevitably generates a byproduct of N, N' -diacetyl cerulosa, and affects the purity of the N-acetyl cerulosa. Disclosure of Invention In order to solve the defects in the prior art, the invention provides a preparation method of N-acetyl cerulosa and application of the N-acetyl cerulosa prepared by the preparation method in fabric dyeing. The above object of the present invention is achieved by the following technical scheme: the preparation method of the N-acetyl blue comprises the following steps: Dispersing N, N '-diacetyl blue in water to obtain a reactant dispersion liquid, adding a composite catalyst to enable the N, N' -diacetyl blue to undergo hydrolysis reaction, then adding a terminator to terminate the reaction and separate out solid, and drying the solid after solid-liquid separation to obtain N-acetylyl blue; the composite catalyst comprises H 2SO4 and aluminum chloride; The terminator includes water at 0-5 ℃. The preparation method of N-acetyl cerulosa provided by the invention has the reaction route shown as the following formula: At present, the preparation method of N-acetylblue in the field mainly follows a reaction route from bottom to top, and the glutamine and the N-acetylglutamine are catalyzed to react to form a ring by a microbial fermentation mode to form the N-acetylblue. The preparation method of N-acetyl cerulosa provided by the invention follows a top-down route, takes N, N '-diacetyl cerulosa as a reactant, can directionally remove one acetyl group from N, N' -diacetyl cerulosa by adopting a specific catalyst, and has the advantages of high reaction rate, high yield and excellent product purity. The reaction in the present application is carried out under the catalysis of a specific catalyst. The inventors of the present application have unexpectedly found that aluminum chloride, which is a lewis acid, can sufficiently amplify the catalytic effect in the strongly acidic environment provided by sulfuric acid, and can provide electrons to participate in the activation of the reactants, thereby reducing the potential barrier of the hydrolysis reaction of N, N' -diacetyl blue. In order to allow the catalyst to directionally remove one acetyl group in the molecule, the mass fraction of each component in the catalyst needs to be accurately controlled. The aluminum chloride of the present application also needs to act synergistically with sulfuric acid. The inventor of the application finds through a great deal of experimental researches that other strong acids such as hydrochloric acid, nitric acid and the like can not replace the effect of sulfuric acid, and can not realize the catalysis of the hydrolysis reaction of N, N '-diacetyl blue by compounding other strong acids with aluminum chloride, and presumably the reasons are that a great deal of halogen ions generated by dissolving hydrochloric acid, hydrobromic acid and the like in water belong to Lewis bases capable of giving electrons, the catalytic activity is reduced due to the easy interaction with Lewis acid, and nitric acid and perchloric acid have strong oxidation effect to influence the reaction tendency of amide bonds in N, N' -diacetyl blue. After the hydrolysis reaction, water at 0-5 ℃ is added as a terminator to terminate the reaction through temperature reduction, and the further hydrolysis of N-acetyl blue can be caused by too high temperature, so that a solid product with a good